Method of artificially aging whisky



C. A. THOMAS ET AL METHOD OF ARTIFICIALLY AGING WHISKY Fi-led Sept. 12,1934 Jan. 7, 1936 Patented Jan. 7, 1936 "UNITED STATE mnrnon oran'rmcmnnr 'AGTNG WHISKY Charles A. Thomas and Carroll JA. Hochwalt,Dayton, Ohio, assignors, by mesne assignments, to Nelson S. Talbott,Dayton, Ohio Application September 12, 1934, Serial lilo. 243,752

16 Claims.

This invention relates to a method of treating green whisky, such asBourbon or rye, and is an r improvement of the process disclosed in ourcopending application Serial No. 703,154, filed December 19, 1933.

An object of the invention is to provide an improved process of treatingwhisky for the effective removal of undesirable taste and odors commonlyknown in the industry as "s1op or green odor. x

' Another .object a process which. removes such .slop or green odors andwhich imparts an increased aroma to the whisky. v

More specifically, an object-of the invention resides in the provisionor a process for hydro- -genating whiskyin the vaporphase in thepresence of a catalyst. In the preferred embodi- -ment, green whisky invapor form is mixed with hydrogen and brought into intimate contact witha catalyst capable of promoting the .reaction of the hydrogen with theconstituents of the whisky to efiect the elimination of deleteriousodors and taste and improve the aroma. vThis step of hydrogenation maybe followed by treatment of i he resulting'product in charred kegsorwith the activated chars disclosed in our copending application abovereferred to in order to lend color to-the whisky and still furtherincrease the aroma thereof. Other objects and advantages of the.invention will appear in the following. description of the preferredembodiment of, the invention illustrated by the accompanying drawing,"of which: Figure. 1 is a vertical sectional view-oi onedormer-apparatus; and

.oitherataivtic treating chamber.

2 is a similar view of a modification C .1 ore drawing,

' 1, indicates a. ondenser for liquetying the weak whisky from theprimary still (not shown)- The weak whisky from the condenser IQisconductedby the pipe ii and into heated water in a doubler still l2.

' dropped The water in. the doubler still l2 may be heated in any. knownor convenient manner but is preferably heated by steam passed throughthe coils l3" positioned in the doubler still. The green whish vaporsfrom the'doubler still l2 are passed through a pipe l4, blower l5; andpipe l6 into a catalytic chamber H. The treating chamber -l'l is partlyfilled with a body :0! water l8 heatedbyfany convenient means, such as asteam coil l9. The water contains a finely divided cataly t such as"powdered nickel of the invention to provide 7 in suspension. The pipe l6extends below the surface of the water and. terminates adjacent thebottom of the chamber ll in a vapor distributing member 20 provided witha plurality of small aperturesv 2|. 5

Prior to passing the green whisky vapors into the treating chamber I1,hydrogen is injected into and mixed with the vapors in. the pipe It bymeans of a pipe 22 connected to a source of hydrogen (not shown). Theblower l5 forces 10 the mixed vapors and hydrogen through the pipe V I6and apertures 2| so that the mixture bubbles up through the heated waterl8 in contact with the suspended catalyst. -The resultant agitation ofthe water aids in keeping the catalyst in sus- 1 5 pension and insuresintimate contact thereof with the mixture of vapors and hydrogen. Thetemperature of the water is preferably maintained above thecondensationtemperature of the whisky vapors so that'hydrogenation takes20 place in the vapor phase. The treated vapors and any excess hydrogencollect above the surface of the water I! injthe treating? chamber l1and are conducted by'a pipe 23 to a condenser where the whisky vaporsare liquefied. 25

From the condenser 24, the excess hydrogen and liquefied whisky areconducted by pipe 25to a hydrogen separating chamber 26 in which thehydrogen collects above the liquid whisky. The

excess hydrogen is returned to the process bye. 30

pipe 21 from the upper portion of the separating chamber 26, a blower 28and pipe 29 connecting with pipe 14 on the low pressure side ,of blowerIS. The liquid whisky in the separating chamber 26 may be conducted by apipe II, a 35 pump 3|, and a pipe 32 to storage means (not shown), whichmay be in charred kegs in order to lend.color to the whisky and furtherincrease its aroma; or the whisky from the separating chamber 26 may besubjected totreatment by an 40,

activated char as" disclosed in applicants above mentioned co -pendingapplication.

The-green whisky vapors may be hydrogenated at temperatures ranging fromthe border line between liquid and vapor phase hydrogen- 4 5 ation,whichis so to. c., up to the boiling point of "the water, which isapproximately C. The temperature of hydrogenation, however, influences.the aroma and flavor or the resulting whisky. The preferred temperatureis approxi- 50 mately 100 c. Attemperatures of so to 95 c.. theresulting product has a somewhat spicy taste 2 and is not quite asaromatic as with the higher temperatures. .At. 100' 0., however, thisspicy taste disappears entirely and the aromatic qual- 55 nickel. Whilefinely divided nickel is preferably ity of the whisky is increased. Theester content goes up approximately 25 parts per one hundred thousand,whereas the original green whisky has only around 10 to 11 parts per onehundred thousand.

It is to be noted that the pressure in the system, or at least that inthe catalytic chamber I'I, may be increased in order to enable thetemperature in the catalytic chamber to be raised to increase the rateof reaction. This, however, introduces operating difiioulties notpresent when substantially atmospheric pressure is used in the cataltyicchamber. Also, at temperatures above 120 C., the ester content increasesto an undesirable extent.

As a specific example of the process, the green whisky vapors from thedoubler still I2 may be under a pressure of approximately three poundsper square inch. The head of catalytic suspension above the distributingmember 20 in the treating chamber I! may be approximately ten feet. Anexcess of hydrogen is admitted into the pipe l4 by the pipe 22 so as toform a. mixture with the green whisky vapors, and the pressure of themixture is raised to approximately eight pounds per square inch by theblower I5 in order to overcome the head of catalyst suspension in thetreating chamber [1. The green whisky'vapors in the pipe l4 may have atemperature of to C., and the water i8 in the treating chamber ispreferably heated to a temperature of approximately 100 C. so as to beat or near the boiling point thereof. Under these conditions the whiskyvapors remain in the vapor phase while contacting the catalyst suspendedin the water. The mixture of whisky vapors and hydrogen leaves theapertures 2| of the distributing member 20 in the" form of small bubblesand intimately contacts the suspended catalyst.

The catalyst preferably employed is finely divided nickel having aparticle size sufliciently small to remain in suspension during thetreating operation and is preferably 200 mesh active ,tion during whichthe whisky vapor and hydro-.

gen are subjected to contact with the catalyst will varywith thecatalyst and cannot be definitely stated. It will be apparent, however,to

those skilled in the art that the vapors must be maintained in contactwith the catalyst a sufficient length of time to remove the deleteriousodors and taste and increase the aroma of the whisky to the-desiredextent.

In Figure 2 is shown a difierent form of catalytic treating device foreffecting vapor phase hydrogenation of green whistky in which the samereference characters are used for portions of the apparatus which areidentical with those of the modification shown in Figure 1. modificationthe pipe l4 from the doubler still has connected thereto the hydrogeninlet pipe 22 and hydrogen return pipe 28 and leads directly to aplurality of treating chambers 33.

e The treating chambers 33 are shown in duplicate in order to increasethe amount of vapor which may be treated, but it is to be understood.

Inthis that a single treating chamber may be provided if it hassufilcient capacity to treat the vapors coming from'the still or, ifnecessary, a larger number of treating chambers may be employed. Thetreating chambers 33 are preferably sur- 5 rounded by heating jackets 34so as to enable the treating chambers to be kept at any desiredtemperature and steam is the heating medium preferably employed. Thetreating chambers 33 contain a. catalyst capable of promoting hydro- 10genation of the green whisky vapor, preferably in finely divided formand supported by an inert material 35.

After passing through the treating chambers 33, the treated vapor andexcess hydrogen are 15 conducted through the pipe 23 to the hydrogenseparating chamber 24 of Figure 1. From the separating chamber, thehydrogen is returned to the process as described with respect toFigure 1. The hydrogenated whisky may then be further treated in charredkegs or with activated char, as also described with respect to themodification shown in Figure 1.

The catalyst alsopreferably used in this modification of the process isfinely divided nickel. The finely divided catalyst is packed with aporous body of inert material such as asbestos, charcoal, coke, pumicestone, or any other porous inert material. This packing acts as asupport for the finely divided nickel, which is preferably 30 a twohundred mesh active nickel, and the catalyst is thoroughly distributedover the inert carrier and rests on ,the surface and in the pots of thematerial. Besides this supporting function, the carrier also acts tobaflle and agitate the vapors, thus aifording repeated and intimatecontact with the catalyst while in the treating chamber.

While finely divided nickel is preferably used as the catalyst in thismodification, the other 40 catalytic materials such as the platinum,iron, chrominum, or copper oxide before mentioned, or any other catalystwhich has the capability of effecting hydrogenation, may be and arecontemplated by our process. As hereinbefore 45 stated, such catalystscarry a small amount of adsorbed oxygen. Also in this modification ofthe process the time of reaction during which the whisky vapor andhydrogen are subjected to contact with the catalyst cannot be definitely50 stated since it will vary with the catalyst used and the temperatureof the treating zone. For the same reasons as in the first describedmodification of the process, the necessary time of reaction will beapparent to thoseskilled in the 55 art.

In this modification of the process. the greenwhisky vapors may behydrogenated at temperatures ranging from the border line between liquidand vapor phase hydrogenation, that is, 90 to 00 C. up to 150 C. Thepreferred temperature however, approximately 120 C. At temperatures of90 to 95 C., the resulting product has a somewhat spicy tasteand is notquite as aromatic as with higher temperatures. With temperatures betweenand 0., however, this spicy taste disappears and the aromatic quality ofthe whisky is increased. As stated with reference to the modification ofFigure 1, the ester content goes up to approximately 25 parts per onehundred from the Ill to H parts per one thousand in the original greenwhisky. Because of greater speed of reaction, the upper limit of thisrange (approximately 120 C.) is preferred. '5

At temperatures above 120 0. the ester content increases quite rapidly,and at hydrogenation temperatures of 150 to 160 C. the resultant productis full of esters and resembles a brandy more than a whisky. Also atthese temperatures the aldehydes develop to a point where they becomeobjectional.

As hereinbefore stated, the present invention is an improvement over theliquid phase process of our above mentioned copending application, andthe vapor phase hydrogenation product is better in every way than theliquid phase product. The

' ester content is raised considerably, and the spicy taste which alwaysoccurs with liquid phase hydrogenation is absent when the green whiskyvapors are hydrogenatedin the vapor phase. The product has amorewhisky-like odor and taste so that when followed by the second stepeither by treatment with the activated char disclosed in our copendingapplication above'referred to, or by aging in a charred barrel, theproduct represents a very, potable whisky. By the vapor phase treatmentof the present invention the aldehydes are increased slightly, which isa desirable feature as [they help to increase the'aroma and taste of thewhisky. This is probably caused by a small percentage of adsorbed oxygenon the nickel catalyst, and even though the reaction is carried on in areduction atmosphereof hydrogen, nevertheless some oxidation occurs,causing formation of aldehydes. By maintaining the temperature ofhydrogenation between approximately and C., the

quantities of aldehydes formed are not objec tionableto thewhiskyalthough if the temperature of hydrogenation is too high, too large aquantity of them forms, which makes the whisky objectionable.Furthermore, the vapor phase process of hydrogenating green whisky doesnot interfere in any way with the regular distilling operations but iscarried on as a continuous step in such distillinggoperations. Ifdesired a portion only of the. green whisky vapors from the doublerstill may be diverted to the hydrogenation process and the remainingportion subjected to the conventional processes.

While we have described our process of vapor phasehydrogenation inconnection with a distilling operation, it is to be understood that theimproved results from vapor phase hydrogenation may be accomplished byinjecting liquid green whisky not taken directly from a still intoheated water and the resultant vapors passed through the vapor phasehydrogenation step. The process may also be performed by directlyheating liquid green whisky and passing the evolved vapors through thehydrogenation step.

Thislast mentioned modification, however, has

details of the invention may be varied within the scope of the followingclaims.

We claim as our invention:

1. The method of artificially aging whisky to improve its odor andtaste, which comprises, the step of passing said whisky in vapor phasewith hydrogen over a hydrogenating catalyst,

and maintaining said whisky in vapor phase during the treatment thereofwith said hydrogen and catalyst.

2. The method of artificially aging whisky to improve its odor andtaste, which comprises, treating the same in vapor phase with hydrogenin the presence of a hydrogenating catalyst, and maintaining'said whiskyin vapor phase during the treatment thereof with said hydrogen andcatalyst. i 1o 3. The methodof artificially aging whisky to improve itsodor and taste, which comprises, the steps of introducing it to a zonecontaining boiling water, leading the vapors thus generated to ahydrogenating zone where they are treated 15 in the presence ofhydrogen, and a hydrogenating catalyst and in finally condensingthe thustreated product.

4. The method of artificially aging green comprises, treating the samein vapor phase with hydrogen in the presence of the hydrogenatingcatalyst at a temperature of from about 95 C. to about 0., andmaintaining said whisky in vapor phase during the treatment thereof 2,with said hydrogen and catalyst.

5. The .method" of artificially aging green whisky to improve its odorand which comprises, passing the whisky in vapor phase and in admixturewith hydrogen over a hyan drogenating catalyst maintained at atemperature of approximately 120 C.

6. A process for artificially aging green whisky to improve its odor andtaste, which comprises, converting the whisky into a vapor 3.3 ofuniform composition by continuously depositing' the liquor onto a bodyofwater maintained at the distillation temperature of the whisky, addinghydrogen to the'resultant vapors and passing the vaporous mixture thusformed into 4; contact withv a hydro'genating catalyst maintained at atemperature adequate to react the hydrogen with constituents ofthejt'aporized phase while in contact with said nickel.

a. In a process of artificially aging whisky to improve its odor andtaste, the, step which comprises, contacting a mixture of whisky vaporand 55 hydrogen with a finely'divided catalyst capable of promoting ahydrogenizing reaction while said catalyst is supported by an inertporous material, and maintaining said whisky;in ,vapor phase whileincontact with said catalyst.

it 9. In a process of artificially aging whisky to improve its odor andtaste, the steps which comprise, passing green whisky vapors andhydrogen through a treating zone containing finely divided nickelsupported by an inert porous material and maintaining said zone at atemperature of substantially 120 C, and maintaining said whisky in vaporphase while in said treat- 10. In a process of manufacturing whiskywherein said whisky is artificially aged to improve its odor and taste,the steps which comprise, distilling said whisky, mixing hydrogen withthe evolved whisky vapors to form a mix- 75 said mixture through atreating zone maintained at a temperature above the liquefication pointof the vapors and containing a catalyst capable of promoting ahydrogenating reaction, condensing said vapors, and subjecting the thusdeoderized whisky to treatment with charred wood containing alcoholsolubles and continuing such treatment until the whisky has beensufliciently aged by said solubles.

12. The method of artificially aging green whisky to improve its odorand taste, which comprises, the steps of treating the green whisky witha finely divided hydrogenating catalyst, in deodorizing the green whiskyby reacting the odoriferous constituents of the whisky in the vaporphase with hydrogen in the presence of the hydrogenating catalyst whilemaintaining the same under pressure sufficient to maintain chemicalhydrogenation of the odoriferous constituents in a substantiallynon-oxidizing atmosphere, continuing the hydrogenation reaction undersaid substantially non-oxidizing atmosphere until the green whisky hasbeen substantially deodorized, maintaining said whisky in vapor phasewhile in the presence of said catalyst, and subjecting the thusdeodorized whisky to treatment with charred wood containing alcoholsolubles and continuing such treatment until the whisky has beensufiiciently aged by said solubles.

13. The method of artificially aging whisky by hydrogenating said whiskyto improve its odor and taste, which comprises, bubbling a mixture ofwhisky vapors and hydrogen through a body of water having a finelydivided catalyst suspended therein, and maintaining the temperature ofthe water sufficiently high to keep the alcohol of the whisky in vaporphase during said hydrogenating.

14. The method of artificially ing whisky by hydrogenating said whiskyto improve its odor and taste, which comprises, contacting a mixture ofwhisky vapors and hydrogen with a catalyst in the presence of water at atemperature above the condensation point of the vapors so as to maintainthe alcohol of the whisky in vapor phase during said hydrogenating.

15. The method of artificially aging whisky by hydrogenating said whiskyto improve its odor and taste, which comprises, introducing a mixture ofwhisky vapors and hydrogen into a treating zone and bubbling saidmixture through a body of water containing a finely divided catalyst,and maintaining said water at the boiling temperature of the water atthe pressure in said zone so as to maintain the alcohol of the whisky invapor phase during said hydrogenat-

